Manufacture of acetylene tetrachlorid.



I J. vom. HANUFAOTUBE 0F AOETYLENE TETRACHL0R11).r

APPLIOATI'OI FILED JUNE 22,1907.

Patented Dec. 29, 1908.

ttoznmao UNITED srnfjnsgnsr OFFICE.

.'IUl/I'US VOI'GT, OF SCHWANHEIM-ON-THE-MAIN, GERMANY, ASSIGNOR TO CHEMISCHE FABRIK GRIESHEIM ELECTRON, OF FRANKFORT-ON-THE-MAIN, GERMANY.

M ANUrAcrUn-E or acErrLENn 'rn'rnncnnonrn I Szpeccation of Letters Patent. 'Application led June 22,`

Patented Dec. 29, 1908.

1907. serial no. .380,316.

To all whom fit may concern: Beit known that I, JULIUs Voler, doctor Tof philosophy, residing at Schw'anheim-on- `chlori on acommercial scale .an its a the-Main, Germany, have yinvented certain new and useful Improvements in the Manu-A Moune rat has, in 1898, (Bullet/ln de la' Societe 0 'im' ue de Paris (3). 19. 1898 page 448 if) state that acetylene and chlorin, when mixed in .a gpseous condition, .can enter into reaction wit out ex lesion occurring if air be entirely excluded i-)rom the operation.

The observation ofMouneyrat does not 110W-,

ever rmit of manufacturin acetylene tion has, so tar, been coniined to the article by J. Nieuwland of Notre Gas Beleuchtung Dame, Indiana, S. A., in theJoumalfr Kepp'ler, 1904,- experi-` ments .are described in which acetylene and v se moved.

-clxlorin have been combined to form acetylenetetracbloridin open vessels without any occurring. These ex eriments "have decreased the 'importance o Mouneyrats observations concerning the necessary exclusion of the air, but Nieuwland has not described anycon'ditions whichhave to be observed to mvariably and with certainty, prevent the explosions and ignitions peculrar to a gaseous mixture of acetylene and chlorin. lNieuwland has stated that he often observed in bis experiments ignitions under circumstances which he could not account for, and this fact can be verified without difficulty by repeating his experiments, and it is evident that the commercial manu- `facture of acet lene tetrachlorid ca'n only be safely undert'a en if the main difficult and danger attendant upon it be entire y` re- The-present invention is basedon the observation, made by me that it is possible to safely manufacture acetylene tetrachlorid lical a oraand obtain good quantitativeyields if the chlon'n and acetylene are, before they come into contact, disseminated through porous or comminuted material which cannot itself enter into reaction with the components, and the mixture of gases thus obtained can by rloperly prolonging the portion of the tube ed with sand, etc. be safely conveyed to the place of reaction and then'the reagents be combi-ned to form acetylene chlorid (with, or without,.the porous or comminuted material being present) by suitable contact substances, or by the action of li ht.

The solid bodies which cane used to prevent explosion and into which each gas is caused to llow, ma be `of the most varied nature," such as san pulverized earthenware, infusorial earth, or other pulverulent material, or it lmay consist of porous clay, or the like. The size of the grains, or pores, may vary from the finest river sand up to .grains of 5 millimeters diameter. A mixture of difierent sizes may also be used. Grains having-a .diameter of from 11,; to 2 millimeters are well suited for carrying out the invention. If a porous material is used the pores referably should not be more than 3 to 4` 'meters in diameter, as otherwise a carbon deposit may be formed by the reactions. Their maxa- -mum size should -be such that they do not. permit the gases igniting, and their minimum size should be such thatthe do not oppose too great a resistance to the o w ofthe gases. The conversion of the gas so obtained into acetylene tetrachlorid can be effected by vari- -ous means. Natural and artificial sources of light, containing chemically active rays, are

both suitable, and simple contact substances, such as iron, antimony, and the like, or liquid intermediaries, or vehicles, (for instance, antimonypentachlorid), are very suitable.

In the accompan drawing, Figure 1 is a vertical sectiona view through an apparatus adapted to carry out the present invention; Fig. 2 is-a similar view of a slightly -dif- 10c ferent form of apparatus.

Referring to Fig. 1, d designates a tube, for example of lead, having its upper end closed by a plug b and bent atc so as to provide an inclined section whichextendsinto a recel-.rer 105 d. A sieve e is arranged within the lower in-A clined portion of the tube, being secured in position by solder or other suitable means, andfrom said sieve tothe point f the tube is filled with grains of gravel and from the 11;

be substituted for the point f to the point g with a mixture of powdered iron and sand. The remaining section of the tube, above the mixture of sand and iron is filled with pure sand. With this upper section of the tube c communicate two nipples or pipes-h., 11 through which, respectively, acetylene and chlorin gases are supplied to the tube. Surrounding a portion of the tube a is a device 7c for cooling the tube and its contents.

Tubes h, c' connected with the main tube a serve respectively to conduct acet lene and chlorin gases to said main tube. he gases mix in the upper, sand-filled section of the tube and as they pass downwardly through the intermediate section, filled as aforesaid with a mixture of-sand and powdered iron, they unite to form acetylene tetrachlorid. This mixing of the gases generates heat and in order'to maintain the apparatus belowpthe boiling point of acetylene tetrachlorid it is necessary to employ the cooling apparatus 7c by which the temperature is preferably maintained at from fifteen to twenty degrees centigrade.

Acetylene tetrachlorid formed as above described percolates through the gravelfilled section of the tube a and passes into the receiver d which is rovided with an outlet. Any suitable re ullating means may be em loyed for contro ling the supply of the ch orin and acetylene gases.

As before stated a porous material may sand in the apparatus. If the ,desired reaction is produced by rays-of light the apparatus must be made of glass and great care taken to so arrange the tube that the entire length thereof is exposed to the action of the light rays. 'In such a construction the section f g of the tube is filled with pure sand. If the tube a is of metal it is necessary to arrange a mercury va or lamp 'v in a transparent cylinder 'v' within the section f g of the tube.

By the means above described it is possible to effect a mixture of acetylene and chlorin in a sin le tube without danger. Said gases may a so be mixed by means of such an apparatus as is illustrated in Fig. 2, referring to which m indicates a container or vessel of any suitable size, form and material, which is provided with a lid or cover n. A tube o leading through the cover n rovides an escape for any excess gas whic may be formed in the vessel, and the lid or cover is also provided with an opening'p through which extends a tube of glass or lead, which tube extends downward below the body of liquid 1' in the vessel m., The liquid f may be any suita body of asbestos ibers able solvent by which chlorin and acetylene may be chemically united, for instance, antimony pentachlorid, or a mixture of antimony pentachlorid and antimony trichlorid, o1' a solution of these substances in acetylene tetrachlorid or other suitable solvent.

Thetube g is entirel filled with porous or comminuted materia which is supported by a sieve s at the lower end of the tube, t being arranged between the sieve. The upper end 'a of the tube is closed and with said tube communicate branch tubes h, i, adapted to respectively admit acetylene and chlorin gases to the tube. The gases mix within the ltube and after passing through the sieve s come into contact with the liquid 1' by which they are absorbed and caused to unite, forming acetylene tetrachlorid.

In the form of aaparatus shown in Fig. 2 it will be seen tiat the reaction takes place within the solution and outside of the tube through which the gases pass, whereas with the apparatus shown in Fig. 1 the reaction occurs in the body of the tube.

Having thus described the invention, what is c aimed is:

1. The herein described process of manufacturing acetylene tetrachlorid, consisting in causin acetylene and chlorin gases to unite whilge contained in a body of granular non-catalytic material.

2. The herein described process of manufacturing acetylene tetrachlorid, consisting in separately introducing chlorin and acetylene gases into abody of orous or comminuted non-catalytic material, and causing said gases to react one on the other while passing through such material.

3. The herein described process of manufacturing acetylene tetrachlorid, consisting in separately introducing chlorin and acetylene gases into a body of porous or comminuted non-catalytic material containin a substance which by contact with sai gases causes them to react one on the other.

4. The herein described process of manufacturing acetylene tetrachlorid, consisting in separately introducing chlorin and acetylene gases into a mixture of granular non catalytic material containing powdered iron.

In testimony whereof, I have signed my name to this specification in the presence of two subscribing witnesses.

JULIUS VOIGT.

Witnesses: i

FRANZ HAssLAoHER, ERWIN DIPPEL. 

